欢迎访问《茶叶科学》,今天是

茶叶科学 ›› 2021, Vol. 41 ›› Issue (5): 717-730.doi: 10.13305/j.cnki.jts.20210804.001

• 研究报告 • 上一篇    下一篇

注射器内分散固相萃取-超高效液相色谱-串联质谱法快速测定茶叶中24种农药残留

马佳丽1,2,3,4, 王晨1,3,4,*, 陈红平1,3,4, 柴云峰1,3,4, 诸力1,3,4, 刘新1,3,4,*   

  1. 1.中国农业科学院茶叶研究所,浙江杭州 310008;
    2.中国农业科学院研究生院,北京 100081;
    3.农业农村部茶叶质量安全控制重点实验室,浙江杭州 310008;
    4.农业农村部茶叶产品质量安全风险评估实验室(杭州),浙江杭州 310008
  • 收稿日期:2021-02-01 修回日期:2021-03-01 出版日期:2021-10-15 发布日期:2021-10-12
  • 通讯作者: *wangchen@tricaas.com;liuxin@tricaas.com
  • 作者简介:马佳丽,女,硕士研究生,主要从事茶叶质量安全研究。
  • 基金资助:
    财政部和农业农村部:国家现代农业产业技术体系(CARS-19)、中国农业科学院创新团队(CAAS-ASTIP-2014-TRICAAS-06)、国家农产品质量安全风险评估项目(GJFP2020001)

Rapid Determination of 24 Pesticide Residues in Tea by in-Syringe Dispersive Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

MA Jiali1,2,3,4, WANG Chen1,3,4,*, CHEN Hongping1,3,4, CHAI Yunfeng1,3,4, ZHU Li1,3,4, LIU Xin1,3,4,*   

  1. 1. Tea Research Institute, Chinese Academy of Agriculture Sciences, Hangzhou 310008, China;
    2. Graduate School, Chinese Academy of Agriculture Sciences, Beijing 100081, China;
    3. Key Laboratory of Tea Quality and Safety Control, Ministry of Agriculture and Rural Affairs, Hangzhou 310008, China;
    4. Laboratory of Quality and Safety Risk Assessment for Tea Products (Hangzhou), Ministry of Agriculture and Rural Affairs, Hangzhou 310008, China
  • Received:2021-02-01 Revised:2021-03-01 Online:2021-10-15 Published:2021-10-12

摘要: 基于茶叶基质特点,开发了注射器内分散固相萃取快速前处理技术,建立了茶叶中24种农药残留超高效液相色谱-串联质谱检测方法。茶叶样品经乙腈提取,无水MgSO4盐析,在设计的注射器装置内以N-丙基乙二胺键合硅胶和石墨化炭黑作为分散吸附剂进行净化,超高效液相色谱-串联质谱法进行检测。在3个添加水平(0.01、0.05、0.5βmg·kg-1)下,红茶和绿茶中24种农药的平均回收率为61.7%~98.8%,相对标准偏差为0.4%~5.5%,准确度和精密度良好。24种农药的红茶和绿茶基质标准工作液线性关系良好,相关系数(R2)均大于0.995,检出限(LOD)和定量限(LOQ)分别为0.05~5.36βμg·kg-1和0.18~17.86βμg·kg-1,该方法具有良好的灵敏度。本方法具有简便快捷、所需仪器少、省时等优势,适用于茶叶中多农药残留的定量检测。

关键词: 茶叶, 超高效液相色谱-串联质谱, 农药残留, 注射器内分散固相萃取

Abstract: Based on the characteristics of tea matrix, a rapid pretreatment technology of in-syringe dispersive solid phase extraction (dSPE) was developed, and an analytical method based on ultra high performance liquid chromatography-tandem mass spectrometry was established for the detection of 24 pesticide residues in tea. Tea samples were extracted using acetonitrile, salted-out with MgSO4, purified with primary secondary amine and graphitized carbon black as dispersive adsorbents in designed syringe devices, and detected by UPLC-MS/MS. Recoveries of 24 pesticides in black and green teas were 61.7%-98.8% at three spiked levels (0.01βmg·kg-1, 0.05βmg·kg-1 and 0.5βmg·kg-1), which indicated high accuracy with the relative standard deviations of 0.4%-5.5%. The calibration curves of 24 pesticides in black and green teas showed good linearity with correlation coefficients (R2) higher than 0.995. The limits of detection (LOD) and the limits of quantitation (LOQ) were 0.05-5.36βμg·kg-1 and 0.18-17.86βμg·kg-1, respectively, which show high sensitivity of this method. Being simple, fast, less instrument required and time-saving, this method is suitable for quantification of multiple pesticide residues in tea.

Key words: tea, ultra high performance liquid chromatography-tandem mass spectrometry, pesticide residues, in-syringe dispersive solid phase extraction

中图分类号: